####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_sad_a _audit_block_doi 10.5517/ccdc.csd.cc113r74 _database_code_depnum_ccdc_archive 'CCDC 956915' loop_ _citation_id _citation_doi _citation_year 1 10.1002/ejic.201301598 2014 _audit_update_record ; 2013-08-21 deposited with the CCDC. 2018-09-03 downloaded from the CCDC. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H62 Cl2 N2 Ni' _chemical_formula_sum 'C40 H62 Cl2 N2 Ni' _chemical_formula_weight 700.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4340(10) _cell_length_b 11.4930(10) _cell_length_c 18.0170(10) _cell_angle_alpha 101.53(2) _cell_angle_beta 91.47(2) _cell_angle_gamma 98.01(2) _cell_volume 1892.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used 9782 _cell_measurement_theta_min 2.312 _cell_measurement_theta_max 26.728 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_F_000 756 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 0.683 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6884 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS-2012/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 446(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode' _diffrn_measurement_device_type 'Smart APEX II Ultra' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 57070 _diffrn_reflns_av_unetI/netI 0.0231 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.155 _diffrn_reflns_theta_max 26.738 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8018 _reflns_number_gt 7082 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX2 v2012.2' _computing_cell_refinement 'SAINT V7.68A' _computing_data_reduction 'SAINT V7.68A' _computing_structure_solution 'SHELXS-2012 (Sheldrick, 2012)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+1.1382P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8018 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0695 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.5000 0.0000 0.5000 0.00865(6) Uani 1 2 d S . P . . Ni2 Ni 1.0000 0.0000 0.0000 0.00995(6) Uani 1 2 d S . P . . Cl1 Cl 0.59623(4) 0.07562(3) 0.40864(2) 0.01360(8) Uani 1 1 d . . . . . Cl2 Cl 1.07673(4) -0.10973(3) 0.07376(2) 0.01533(8) Uani 1 1 d . . . . . N1 N 0.50819(12) 0.23236(10) 0.61074(6) 0.0098(2) Uani 1 1 d . . . . . N2 N 1.07847(12) 0.21023(10) 0.12904(6) 0.0108(2) Uani 1 1 d . . . . . C1 C 0.45069(14) 0.14984(12) 0.55230(8) 0.0097(3) Uani 1 1 d . . . . . C2 C 0.41546(15) 0.32991(13) 0.64003(8) 0.0131(3) Uani 1 1 d . . . . . C3 C 0.27225(15) 0.27412(13) 0.59695(8) 0.0136(3) Uani 1 1 d . . . . . H3A H 0.2251 0.3355 0.5810 0.016 Uiso 1 1 calc R U . . . H3B H 0.2094 0.2344 0.6290 0.016 Uiso 1 1 calc R U . . . C4 C 0.30731(15) 0.18304(12) 0.52771(8) 0.0119(3) Uani 1 1 d . . . . . C5 C 0.47875(16) 0.44924(13) 0.62100(9) 0.0179(3) Uani 1 1 d . . . . . H5A H 0.4871 0.4391 0.5672 0.027 Uiso 1 1 calc R U . . . H5B H 0.5719 0.4757 0.6463 0.027 Uiso 1 1 calc R U . . . H5C H 0.4171 0.5081 0.6375 0.027 Uiso 1 1 calc R U . . . C6 C 0.40071(17) 0.34887(14) 0.72550(8) 0.0183(3) Uani 1 1 d . . . . . H6A H 0.3370 0.4065 0.7406 0.027 Uiso 1 1 calc R U . . . H6B H 0.4931 0.3780 0.7512 0.027 Uiso 1 1 calc R U . . . H6C H 0.3627 0.2741 0.7385 0.027 Uiso 1 1 calc R U . . . C7 C 0.32981(16) 0.23972(13) 0.45737(8) 0.0157(3) Uani 1 1 d . . . . . H7A H 0.3536 0.1807 0.4157 0.024 Uiso 1 1 calc R U . . . H7B H 0.4065 0.3060 0.4686 0.024 Uiso 1 1 calc R U . . . H7C H 0.2433 0.2678 0.4440 0.024 Uiso 1 1 calc R U . . . C8 C 0.18771(16) 0.07563(13) 0.50689(9) 0.0161(3) Uani 1 1 d . . . . . H8A H 0.1007 0.1027 0.4933 0.024 Uiso 1 1 calc R U . . . H8B H 0.1731 0.0378 0.5496 0.024 Uiso 1 1 calc R U . . . H8C H 0.2144 0.0190 0.4647 0.024 Uiso 1 1 calc R U . . . C9 C 0.65422(14) 0.24553(12) 0.64512(8) 0.0106(3) Uani 1 1 d . . . . . C10 C 0.67750(15) 0.20609(12) 0.71350(8) 0.0125(3) Uani 1 1 d . . . . . C11 C 0.81467(16) 0.23419(13) 0.74917(8) 0.0159(3) Uani 1 1 d . . . . . H11 H 0.8315 0.2089 0.7941 0.019 Uiso 1 1 calc R U . . . C12 C 0.92595(16) 0.29856(14) 0.71945(9) 0.0172(3) Uani 1 1 d . . . . . H12 H 1.0158 0.3184 0.7449 0.021 Uiso 1 1 calc R U . . . C13 C 0.90267(16) 0.33315(13) 0.65154(9) 0.0156(3) Uani 1 1 d . . . . . H13 H 0.9785 0.3752 0.6313 0.019 Uiso 1 1 calc R U . . . C14 C 0.76873(15) 0.30678(12) 0.61232(8) 0.0119(3) Uani 1 1 d . . . . . C15 C 0.56751(16) 0.12687(13) 0.74912(8) 0.0149(3) Uani 1 1 d . . . . . H15 H 0.4757 0.1142 0.7198 0.018 Uiso 1 1 calc R U . . . C16 C 0.54499(18) 0.18096(16) 0.83248(9) 0.0230(3) Uani 1 1 d . . . . . H16A H 0.5203 0.2601 0.8363 0.034 Uiso 1 1 calc R U . . . H16B H 0.6317 0.1854 0.8626 0.034 Uiso 1 1 calc R U . . . H16C H 0.4689 0.1311 0.8506 0.034 Uiso 1 1 calc R U . . . C17 C 0.61829(17) 0.00477(14) 0.74648(9) 0.0205(3) Uani 1 1 d . . . . . H17A H 0.6434 -0.0270 0.6959 0.031 Uiso 1 1 calc R U . . . H17B H 0.5426 -0.0498 0.7610 0.031 Uiso 1 1 calc R U . . . H17C H 0.7005 0.0149 0.7809 0.031 Uiso 1 1 calc R U . . . C18 C 0.76235(15) 0.34026(13) 0.53465(8) 0.0136(3) Uani 1 1 d . . . . . H18 H 0.6651 0.3138 0.5115 0.016 Uiso 1 1 calc R U . . . C19 C 0.86799(16) 0.27642(14) 0.48343(8) 0.0169(3) Uani 1 1 d . . . . . H19A H 0.8533 0.2875 0.4325 0.025 Uiso 1 1 calc R U . . . H19B H 0.8522 0.1922 0.4839 0.025 Uiso 1 1 calc R U . . . H19C H 0.9645 0.3097 0.5019 0.025 Uiso 1 1 calc R U . . . C20 C 0.80101(17) 0.47609(14) 0.53915(10) 0.0203(3) Uani 1 1 d . . . . . H20A H 0.8978 0.5022 0.5596 0.030 Uiso 1 1 calc R U . . . H20B H 0.7370 0.5180 0.5714 0.030 Uiso 1 1 calc R U . . . H20C H 0.7923 0.4929 0.4893 0.030 Uiso 1 1 calc R U . . . C21 C 1.10736(15) 0.13858(12) 0.06650(8) 0.0109(3) Uani 1 1 d . . . . . C22 C 1.20840(15) 0.29429(13) 0.17274(8) 0.0137(3) Uani 1 1 d . . . . . C23 C 1.33101(15) 0.24636(14) 0.12781(8) 0.0151(3) Uani 1 1 d . . . . . H23A H 1.3761 0.1941 0.1541 0.018 Uiso 1 1 calc R U . . . H23B H 1.4029 0.3122 0.1215 0.018 Uiso 1 1 calc R U . . . C24 C 1.26420(15) 0.17651(13) 0.05050(8) 0.0138(3) Uani 1 1 d . . . . . C25 C 1.19845(17) 0.42575(13) 0.17297(9) 0.0183(3) Uani 1 1 d . . . . . H25A H 1.1905 0.4367 0.1217 0.028 Uiso 1 1 calc R U . . . H25B H 1.2830 0.4753 0.1985 0.028 Uiso 1 1 calc R U . . . H25C H 1.1156 0.4479 0.1989 0.028 Uiso 1 1 calc R U . . . C26 C 1.22031(17) 0.27941(14) 0.25481(8) 0.0183(3) Uani 1 1 d . . . . . H26A H 1.2219 0.1964 0.2558 0.027 Uiso 1 1 calc R U . . . H26B H 1.1395 0.3059 0.2809 0.027 Uiso 1 1 calc R U . . . H26C H 1.3071 0.3265 0.2794 0.027 Uiso 1 1 calc R U . . . C27 C 1.26479(16) 0.25963(14) -0.00721(8) 0.0173(3) Uani 1 1 d . . . . . H27A H 1.3618 0.2856 -0.0181 0.026 Uiso 1 1 calc R U . . . H27B H 1.2205 0.3283 0.0138 0.026 Uiso 1 1 calc R U . . . H27C H 1.2124 0.2166 -0.0532 0.026 Uiso 1 1 calc R U . . . C28 C 1.34420(16) 0.07219(14) 0.01825(9) 0.0187(3) Uani 1 1 d . . . . . H28A H 1.2971 0.0283 -0.0289 0.028 Uiso 1 1 calc R U . . . H28B H 1.3447 0.0198 0.0536 0.028 Uiso 1 1 calc R U . . . H28C H 1.4411 0.1030 0.0099 0.028 Uiso 1 1 calc R U . . . C29 C 0.93804(15) 0.22158(12) 0.16091(8) 0.0116(3) Uani 1 1 d . . . . . C30 C 0.89238(15) 0.15811(13) 0.21753(8) 0.0134(3) Uani 1 1 d . . . . . C31 C 0.77129(16) 0.18688(14) 0.25600(9) 0.0181(3) Uani 1 1 d . . . . . H31 H 0.7407 0.1464 0.2939 0.022 Uiso 1 1 calc R U . . . C32 C 0.69604(17) 0.27372(15) 0.23925(9) 0.0200(3) Uani 1 1 d . . . . . H32 H 0.6180 0.2939 0.2670 0.024 Uiso 1 1 calc R U . . . C33 C 0.73741(16) 0.33047(14) 0.18105(9) 0.0178(3) Uani 1 1 d . . . . . H33 H 0.6837 0.3866 0.1687 0.021 Uiso 1 1 calc R U . . . C34 C 0.85725(16) 0.30642(13) 0.14001(8) 0.0139(3) Uani 1 1 d . . . . . C35 C 0.95836(16) 0.05293(13) 0.23596(8) 0.0143(3) Uani 1 1 d . . . . . H35 H 1.0445 0.0443 0.2072 0.017 Uiso 1 1 calc R U . . . C36 C 0.84912(17) -0.06146(14) 0.21060(9) 0.0189(3) Uani 1 1 d . . . . . H36A H 0.8167 -0.0678 0.1588 0.028 Uiso 1 1 calc R U . . . H36B H 0.7689 -0.0578 0.2423 0.028 Uiso 1 1 calc R U . . . H36C H 0.8935 -0.1303 0.2149 0.028 Uiso 1 1 calc R U . . . C37 C 0.99899(18) 0.06632(15) 0.32054(8) 0.0202(3) Uani 1 1 d . . . . . H37A H 1.0459 0.0001 0.3278 0.030 Uiso 1 1 calc R U . . . H37B H 0.9139 0.0670 0.3487 0.030 Uiso 1 1 calc R U . . . H37C H 1.0626 0.1402 0.3381 0.030 Uiso 1 1 calc R U . . . C38 C 0.88264(16) 0.36716(13) 0.07265(8) 0.0159(3) Uani 1 1 d . . . . . H38 H 0.9681 0.3420 0.0482 0.019 Uiso 1 1 calc R U . . . C39 C 0.75359(18) 0.32666(15) 0.01511(9) 0.0219(3) Uani 1 1 d . . . . . H39A H 0.7758 0.3540 -0.0308 0.033 Uiso 1 1 calc R U . . . H39B H 0.6719 0.3600 0.0359 0.033 Uiso 1 1 calc R U . . . H39C H 0.7324 0.2406 0.0042 0.033 Uiso 1 1 calc R U . . . C40 C 0.90458(18) 0.50520(14) 0.09473(9) 0.0217(3) Uani 1 1 d . . . . . H40A H 0.9200 0.5380 0.0501 0.033 Uiso 1 1 calc R U . . . H40B H 0.9864 0.5325 0.1298 0.033 Uiso 1 1 calc R U . . . H40C H 0.8209 0.5312 0.1181 0.033 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01017(12) 0.00751(12) 0.00824(12) 0.00124(9) 0.00066(9) 0.00175(9) Ni2 0.01053(13) 0.01071(13) 0.00816(12) 0.00094(9) -0.00017(9) 0.00153(9) Cl1 0.01571(17) 0.01395(16) 0.01150(16) 0.00430(13) 0.00211(12) 0.00069(13) Cl2 0.01852(18) 0.01600(17) 0.01236(16) 0.00380(13) -0.00066(13) 0.00462(13) N1 0.0086(6) 0.0095(5) 0.0119(6) 0.0023(4) 0.0015(4) 0.0026(4) N2 0.0096(6) 0.0120(6) 0.0107(6) 0.0025(5) -0.0009(4) 0.0012(5) C1 0.0103(6) 0.0099(6) 0.0102(6) 0.0056(5) 0.0018(5) 0.0006(5) C2 0.0111(7) 0.0117(7) 0.0158(7) -0.0012(5) 0.0002(5) 0.0048(5) C3 0.0104(7) 0.0135(7) 0.0168(7) 0.0012(6) 0.0007(5) 0.0035(5) C4 0.0107(7) 0.0111(7) 0.0140(7) 0.0020(5) -0.0007(5) 0.0028(5) C5 0.0159(7) 0.0107(7) 0.0259(8) -0.0006(6) 0.0006(6) 0.0041(6) C6 0.0165(7) 0.0209(8) 0.0155(7) -0.0034(6) 0.0012(6) 0.0066(6) C7 0.0178(7) 0.0143(7) 0.0163(7) 0.0043(6) -0.0017(6) 0.0052(6) C8 0.0129(7) 0.0142(7) 0.0206(7) 0.0026(6) -0.0036(6) 0.0022(6) C9 0.0092(7) 0.0091(6) 0.0121(7) -0.0017(5) -0.0012(5) 0.0026(5) C10 0.0130(7) 0.0113(7) 0.0120(7) -0.0011(5) 0.0004(5) 0.0033(5) C11 0.0160(7) 0.0186(7) 0.0130(7) 0.0027(6) -0.0021(6) 0.0038(6) C12 0.0108(7) 0.0191(8) 0.0196(8) -0.0006(6) -0.0041(6) 0.0030(6) C13 0.0107(7) 0.0151(7) 0.0200(7) 0.0017(6) 0.0017(6) 0.0008(6) C14 0.0127(7) 0.0079(6) 0.0148(7) -0.0002(5) 0.0014(5) 0.0038(5) C15 0.0138(7) 0.0195(7) 0.0110(7) 0.0039(6) -0.0017(5) 0.0008(6) C16 0.0188(8) 0.0373(10) 0.0123(7) 0.0050(7) 0.0005(6) 0.0027(7) C17 0.0205(8) 0.0198(8) 0.0214(8) 0.0084(6) -0.0068(6) -0.0008(6) C18 0.0114(7) 0.0127(7) 0.0170(7) 0.0045(6) 0.0004(5) 0.0007(5) C19 0.0151(7) 0.0179(7) 0.0170(7) 0.0030(6) 0.0033(6) 0.0004(6) C20 0.0198(8) 0.0151(7) 0.0283(8) 0.0093(6) 0.0044(6) 0.0027(6) C21 0.0121(7) 0.0119(7) 0.0107(6) 0.0057(5) 0.0003(5) 0.0042(5) C22 0.0111(7) 0.0141(7) 0.0133(7) -0.0002(5) -0.0024(5) -0.0014(5) C23 0.0108(7) 0.0178(7) 0.0165(7) 0.0037(6) -0.0005(6) 0.0011(6) C24 0.0126(7) 0.0153(7) 0.0132(7) 0.0023(6) 0.0018(5) 0.0019(6) C25 0.0185(8) 0.0135(7) 0.0209(8) 0.0009(6) -0.0022(6) -0.0002(6) C26 0.0175(8) 0.0204(8) 0.0142(7) -0.0001(6) -0.0032(6) -0.0011(6) C27 0.0165(7) 0.0199(8) 0.0153(7) 0.0051(6) 0.0022(6) -0.0007(6) C28 0.0135(7) 0.0199(8) 0.0225(8) 0.0023(6) 0.0059(6) 0.0042(6) C29 0.0097(7) 0.0132(7) 0.0099(6) -0.0020(5) -0.0005(5) 0.0008(5) C30 0.0125(7) 0.0157(7) 0.0100(6) -0.0004(5) -0.0009(5) 0.0000(6) C31 0.0174(8) 0.0211(8) 0.0153(7) 0.0034(6) 0.0042(6) 0.0015(6) C32 0.0147(7) 0.0245(8) 0.0199(8) -0.0004(6) 0.0062(6) 0.0057(6) C33 0.0164(7) 0.0168(7) 0.0201(8) 0.0003(6) 0.0000(6) 0.0068(6) C34 0.0138(7) 0.0133(7) 0.0126(7) -0.0014(5) -0.0023(5) 0.0012(6) C35 0.0144(7) 0.0175(7) 0.0111(7) 0.0037(6) 0.0021(5) 0.0020(6) C36 0.0193(8) 0.0182(8) 0.0197(8) 0.0051(6) 0.0044(6) 0.0015(6) C37 0.0217(8) 0.0273(9) 0.0127(7) 0.0070(6) 0.0010(6) 0.0037(7) C38 0.0177(7) 0.0176(7) 0.0135(7) 0.0027(6) 0.0000(6) 0.0073(6) C39 0.0223(8) 0.0279(9) 0.0161(7) 0.0014(6) -0.0037(6) 0.0105(7) C40 0.0272(9) 0.0183(8) 0.0221(8) 0.0069(6) 0.0012(7) 0.0079(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.9150(14) . ? Ni1 C1 1.9150(14) 2_656 ? Ni1 Cl1 2.1720(5) . ? Ni1 Cl1 2.1720(5) 2_656 ? Ni2 C21 1.9296(15) . ? Ni2 C21 1.9297(15) 2_755 ? Ni2 Cl2 2.1808(5) 2_755 ? Ni2 Cl2 2.1808(5) . ? N1 C1 1.3154(18) . ? N1 C9 1.4714(18) . ? N1 C2 1.5367(17) . ? N2 C21 1.3150(18) . ? N2 C29 1.4693(18) . ? N2 C22 1.5402(18) . ? C1 C4 1.5336(19) . ? C2 C6 1.524(2) . ? C2 C5 1.525(2) . ? C2 C3 1.531(2) . ? C3 C4 1.535(2) . ? C4 C8 1.531(2) . ? C4 C7 1.5430(19) . ? C9 C14 1.414(2) . ? C9 C10 1.4173(19) . ? C10 C11 1.396(2) . ? C10 C15 1.524(2) . ? C11 C12 1.381(2) . ? C12 C13 1.381(2) . ? C13 C14 1.396(2) . ? C14 C18 1.5256(19) . ? C15 C17 1.537(2) . ? C15 C16 1.539(2) . ? C18 C19 1.537(2) . ? C18 C20 1.538(2) . ? C21 C24 1.5345(19) . ? C22 C26 1.525(2) . ? C22 C25 1.526(2) . ? C22 C23 1.531(2) . ? C23 C24 1.533(2) . ? C24 C28 1.530(2) . ? C24 C27 1.546(2) . ? C29 C30 1.411(2) . ? C29 C34 1.419(2) . ? C30 C31 1.396(2) . ? C30 C35 1.523(2) . ? C31 C32 1.378(2) . ? C32 C33 1.379(2) . ? C33 C34 1.396(2) . ? C34 C38 1.525(2) . ? C35 C37 1.5339(19) . ? C35 C36 1.535(2) . ? C38 C39 1.536(2) . ? C38 C40 1.539(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 C1 180.0 . 2_656 ? C1 Ni1 Cl1 93.82(4) . . ? C1 Ni1 Cl1 86.18(4) 2_656 . ? C1 Ni1 Cl1 86.18(4) . 2_656 ? C1 Ni1 Cl1 93.82(4) 2_656 2_656 ? Cl1 Ni1 Cl1 180.0 . 2_656 ? C21 Ni2 C21 180.0 . 2_755 ? C21 Ni2 Cl2 92.13(4) . 2_755 ? C21 Ni2 Cl2 87.87(4) 2_755 2_755 ? C21 Ni2 Cl2 87.87(4) . . ? C21 Ni2 Cl2 92.13(4) 2_755 . ? Cl2 Ni2 Cl2 180.0 2_755 . ? C1 N1 C9 126.62(12) . . ? C1 N1 C2 115.04(11) . . ? C9 N1 C2 118.09(11) . . ? C21 N2 C29 128.05(12) . . ? C21 N2 C22 115.36(12) . . ? C29 N2 C22 116.57(11) . . ? N1 C1 C4 108.56(12) . . ? N1 C1 Ni1 134.40(10) . . ? C4 C1 Ni1 116.85(10) . . ? C6 C2 C5 108.46(12) . . ? C6 C2 C3 111.00(12) . . ? C5 C2 C3 113.72(12) . . ? C6 C2 N1 112.48(12) . . ? C5 C2 N1 110.60(11) . . ? C3 C2 N1 100.50(11) . . ? C2 C3 C4 106.46(11) . . ? C8 C4 C1 113.66(11) . . ? C8 C4 C3 111.47(12) . . ? C1 C4 C3 103.41(11) . . ? C8 C4 C7 107.95(12) . . ? C1 C4 C7 108.40(11) . . ? C3 C4 C7 111.94(12) . . ? C14 C9 C10 120.63(13) . . ? C14 C9 N1 118.89(12) . . ? C10 C9 N1 120.27(12) . . ? C11 C10 C9 118.21(13) . . ? C11 C10 C15 116.29(13) . . ? C9 C10 C15 125.34(13) . . ? C12 C11 C10 121.68(14) . . ? C11 C12 C13 119.41(14) . . ? C12 C13 C14 121.95(14) . . ? C13 C14 C9 118.01(13) . . ? C13 C14 C18 116.09(13) . . ? C9 C14 C18 125.78(13) . . ? C10 C15 C17 109.20(12) . . ? C10 C15 C16 113.06(13) . . ? C17 C15 C16 107.73(13) . . ? C14 C18 C19 109.67(12) . . ? C14 C18 C20 112.62(12) . . ? C19 C18 C20 107.98(12) . . ? N2 C21 C24 107.83(12) . . ? N2 C21 Ni2 133.69(11) . . ? C24 C21 Ni2 118.37(10) . . ? C26 C22 C25 108.32(12) . . ? C26 C22 C23 111.17(12) . . ? C25 C22 C23 114.04(12) . . ? C26 C22 N2 111.05(12) . . ? C25 C22 N2 111.61(12) . . ? C23 C22 N2 100.55(11) . . ? C22 C23 C24 106.51(12) . . ? C28 C24 C23 111.66(12) . . ? C28 C24 C21 114.46(12) . . ? C23 C24 C21 103.62(11) . . ? C28 C24 C27 108.61(12) . . ? C23 C24 C27 110.89(12) . . ? C21 C24 C27 107.48(12) . . ? C30 C29 C34 120.76(13) . . ? C30 C29 N2 119.87(12) . . ? C34 C29 N2 119.01(12) . . ? C31 C30 C29 118.27(14) . . ? C31 C30 C35 116.78(13) . . ? C29 C30 C35 124.77(13) . . ? C32 C31 C30 121.63(14) . . ? C31 C32 C33 119.43(14) . . ? C32 C33 C34 122.16(14) . . ? C33 C34 C29 117.55(13) . . ? C33 C34 C38 116.51(13) . . ? C29 C34 C38 125.77(13) . . ? C30 C35 C37 113.74(12) . . ? C30 C35 C36 108.18(12) . . ? C37 C35 C36 108.36(12) . . ? C34 C38 C39 109.35(13) . . ? C34 C38 C40 113.46(12) . . ? C39 C38 C40 108.16(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N1 C1 C4 -170.41(12) . . . . ? C2 N1 C1 C4 3.71(15) . . . . ? C9 N1 C1 Ni1 15.0(2) . . . . ? C2 N1 C1 Ni1 -170.92(10) . . . . ? C1 N1 C2 C6 129.80(13) . . . . ? C9 N1 C2 C6 -55.55(16) . . . . ? C1 N1 C2 C5 -108.76(14) . . . . ? C9 N1 C2 C5 65.89(15) . . . . ? C1 N1 C2 C3 11.69(15) . . . . ? C9 N1 C2 C3 -173.66(11) . . . . ? C6 C2 C3 C4 -141.02(12) . . . . ? C5 C2 C3 C4 96.35(14) . . . . ? N1 C2 C3 C4 -21.84(14) . . . . ? N1 C1 C4 C8 -138.61(12) . . . . ? Ni1 C1 C4 C8 37.09(15) . . . . ? N1 C1 C4 C3 -17.59(14) . . . . ? Ni1 C1 C4 C3 158.11(9) . . . . ? N1 C1 C4 C7 101.36(13) . . . . ? Ni1 C1 C4 C7 -82.93(12) . . . . ? C2 C3 C4 C8 147.08(12) . . . . ? C2 C3 C4 C1 24.58(14) . . . . ? C2 C3 C4 C7 -91.90(14) . . . . ? C1 N1 C9 C14 83.07(17) . . . . ? C2 N1 C9 C14 -90.89(15) . . . . ? C1 N1 C9 C10 -102.05(16) . . . . ? C2 N1 C9 C10 83.98(16) . . . . ? C14 C9 C10 C11 2.9(2) . . . . ? N1 C9 C10 C11 -171.91(12) . . . . ? C14 C9 C10 C15 -172.35(13) . . . . ? N1 C9 C10 C15 12.9(2) . . . . ? C9 C10 C11 C12 0.0(2) . . . . ? C15 C10 C11 C12 175.65(14) . . . . ? C10 C11 C12 C13 -2.0(2) . . . . ? C11 C12 C13 C14 1.1(2) . . . . ? C12 C13 C14 C9 1.7(2) . . . . ? C12 C13 C14 C18 -174.51(13) . . . . ? C10 C9 C14 C13 -3.7(2) . . . . ? N1 C9 C14 C13 171.19(12) . . . . ? C10 C9 C14 C18 172.08(13) . . . . ? N1 C9 C14 C18 -13.1(2) . . . . ? C11 C10 C15 C17 -61.86(16) . . . . ? C9 C10 C15 C17 113.45(15) . . . . ? C11 C10 C15 C16 58.05(17) . . . . ? C9 C10 C15 C16 -126.64(15) . . . . ? C13 C14 C18 C19 58.03(16) . . . . ? C9 C14 C18 C19 -117.79(15) . . . . ? C13 C14 C18 C20 -62.23(17) . . . . ? C9 C14 C18 C20 121.94(15) . . . . ? C29 N2 C21 C24 169.85(12) . . . . ? C22 N2 C21 C24 -8.57(15) . . . . ? C29 N2 C21 Ni2 -14.1(2) . . . . ? C22 N2 C21 Ni2 167.49(10) . . . . ? C21 N2 C22 C26 -124.95(13) . . . . ? C29 N2 C22 C26 56.44(16) . . . . ? C21 N2 C22 C25 114.08(14) . . . . ? C29 N2 C22 C25 -64.53(15) . . . . ? C21 N2 C22 C23 -7.23(15) . . . . ? C29 N2 C22 C23 174.17(11) . . . . ? C26 C22 C23 C24 137.39(12) . . . . ? C25 C22 C23 C24 -99.80(14) . . . . ? N2 C22 C23 C24 19.76(14) . . . . ? C22 C23 C24 C28 -148.73(12) . . . . ? C22 C23 C24 C21 -25.04(14) . . . . ? C22 C23 C24 C27 89.99(14) . . . . ? N2 C21 C24 C28 142.59(12) . . . . ? Ni2 C21 C24 C28 -34.17(15) . . . . ? N2 C21 C24 C23 20.75(14) . . . . ? Ni2 C21 C24 C23 -156.01(9) . . . . ? N2 C21 C24 C27 -96.70(13) . . . . ? Ni2 C21 C24 C27 86.54(12) . . . . ? C21 N2 C29 C30 96.08(17) . . . . ? C22 N2 C29 C30 -85.51(16) . . . . ? C21 N2 C29 C34 -90.67(17) . . . . ? C22 N2 C29 C34 87.73(15) . . . . ? C34 C29 C30 C31 -4.3(2) . . . . ? N2 C29 C30 C31 168.80(13) . . . . ? C34 C29 C30 C35 170.57(13) . . . . ? N2 C29 C30 C35 -16.3(2) . . . . ? C29 C30 C31 C32 0.8(2) . . . . ? C35 C30 C31 C32 -174.55(14) . . . . ? C30 C31 C32 C33 2.7(2) . . . . ? C31 C32 C33 C34 -2.6(2) . . . . ? C32 C33 C34 C29 -0.9(2) . . . . ? C32 C33 C34 C38 174.62(14) . . . . ? C30 C29 C34 C33 4.4(2) . . . . ? N2 C29 C34 C33 -168.81(13) . . . . ? C30 C29 C34 C38 -170.67(13) . . . . ? N2 C29 C34 C38 16.1(2) . . . . ? C31 C30 C35 C37 -55.94(18) . . . . ? C29 C30 C35 C37 129.10(15) . . . . ? C31 C30 C35 C36 64.50(16) . . . . ? C29 C30 C35 C36 -110.46(15) . . . . ? C33 C34 C38 C39 -60.52(17) . . . . ? C29 C34 C38 C39 114.57(16) . . . . ? C33 C34 C38 C40 60.31(18) . . . . ? C29 C34 C38 C40 -124.60(15) . . . . ? _refine_diff_density_max 0.439 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.050 _shelxl_version_number 2013-4 _shelx_res_file ; REM Solution 1 R1 0.084 Rweak 0.005, Alpha = 0.0650 in P-1 REM Formula: C39 N3 Cl2 Ni TITL sad in P-1 CELL 0.71073 9.434 11.493 18.017 101.53 91.47 98.01 ZERR 2.0 0.001 0.001 0.001 0.02 0.02 0.02 LATT 1 SFAC C H N CL NI UNIT 80 124 4 4 2 TEMP 173.000 L.S. 10 BOND LIST 4 conf acta omit 0 7 7 omit -6 6 0 FMAP 2 PLAN 20 WGHT 0.031600 1.138200 FVAR 0.54470 NI1 5 0.500000 0.000000 0.500000 10.50000 0.01017 0.00751 = 0.00824 0.00124 0.00066 0.00175 NI2 5 1.000000 0.000000 0.000000 10.50000 0.01053 0.01071 = 0.00816 0.00094 -0.00017 0.00153 CL1 4 0.596229 0.075618 0.408642 11.00000 0.01571 0.01395 = 0.01150 0.00430 0.00211 0.00069 CL2 4 1.076734 -0.109735 0.073762 11.00000 0.01852 0.01600 = 0.01236 0.00380 -0.00066 0.00462 N1 3 0.508193 0.232357 0.610737 11.00000 0.00859 0.00947 = 0.01185 0.00231 0.00149 0.00258 N2 3 1.078469 0.210234 0.129037 11.00000 0.00957 0.01196 = 0.01074 0.00245 -0.00085 0.00125 C1 1 0.450687 0.149843 0.552300 11.00000 0.01030 0.00990 = 0.01023 0.00555 0.00178 0.00063 C2 1 0.415462 0.329910 0.640034 11.00000 0.01108 0.01165 = 0.01582 -0.00119 0.00017 0.00476 C3 1 0.272251 0.274124 0.596953 11.00000 0.01037 0.01346 = 0.01679 0.00118 0.00066 0.00351 AFIX 23 H3A 2 0.225128 0.335534 0.580964 11.00000 -1.20000 H3B 2 0.209391 0.234355 0.628976 11.00000 -1.20000 AFIX 0 C4 1 0.307312 0.183040 0.527714 11.00000 0.01068 0.01111 = 0.01403 0.00205 -0.00073 0.00284 C5 1 0.478753 0.449239 0.620999 11.00000 0.01590 0.01074 = 0.02590 -0.00058 0.00060 0.00410 AFIX 137 H5A 2 0.487105 0.439106 0.567172 11.00000 -1.50000 H5B 2 0.571862 0.475667 0.646317 11.00000 -1.50000 H5C 2 0.417138 0.508068 0.637523 11.00000 -1.50000 AFIX 0 C6 1 0.400706 0.348871 0.725497 11.00000 0.01649 0.02091 = 0.01549 -0.00342 0.00116 0.00660 AFIX 137 H6A 2 0.336995 0.406513 0.740624 11.00000 -1.50000 H6B 2 0.493095 0.377965 0.751163 11.00000 -1.50000 H6C 2 0.362734 0.274079 0.738534 11.00000 -1.50000 AFIX 0 C7 1 0.329814 0.239720 0.457371 11.00000 0.01777 0.01430 = 0.01628 0.00431 -0.00174 0.00524 AFIX 137 H7A 2 0.353561 0.180670 0.415707 11.00000 -1.50000 H7B 2 0.406536 0.305951 0.468601 11.00000 -1.50000 H7C 2 0.243345 0.267801 0.444041 11.00000 -1.50000 AFIX 0 C8 1 0.187711 0.075627 0.506887 11.00000 0.01293 0.01419 = 0.02055 0.00257 -0.00364 0.00215 AFIX 137 H8A 2 0.100699 0.102682 0.493310 11.00000 -1.50000 H8B 2 0.173061 0.037821 0.549571 11.00000 -1.50000 H8C 2 0.214361 0.019010 0.464719 11.00000 -1.50000 AFIX 0 C9 1 0.654219 0.245529 0.645121 11.00000 0.00921 0.00913 = 0.01210 -0.00174 -0.00118 0.00262 C10 1 0.677499 0.206091 0.713504 11.00000 0.01303 0.01133 = 0.01198 -0.00107 0.00042 0.00331 C11 1 0.814671 0.234192 0.749168 11.00000 0.01605 0.01865 = 0.01301 0.00274 -0.00214 0.00380 AFIX 43 H11 2 0.831520 0.208912 0.794086 11.00000 -1.20000 AFIX 0 C12 1 0.925946 0.298557 0.719446 11.00000 0.01075 0.01915 = 0.01960 -0.00065 -0.00408 0.00302 AFIX 43 H12 2 1.015756 0.318442 0.744920 11.00000 -1.20000 AFIX 0 C13 1 0.902675 0.333147 0.651539 11.00000 0.01066 0.01507 = 0.01996 0.00172 0.00171 0.00075 AFIX 43 H13 2 0.978459 0.375240 0.631344 11.00000 -1.20000 AFIX 0 C14 1 0.768732 0.306783 0.612320 11.00000 0.01270 0.00788 = 0.01483 -0.00018 0.00138 0.00381 C15 1 0.567508 0.126875 0.749119 11.00000 0.01384 0.01950 = 0.01100 0.00386 -0.00168 0.00081 AFIX 13 H15 2 0.475723 0.114183 0.719813 11.00000 -1.20000 AFIX 0 C16 1 0.544985 0.180965 0.832481 11.00000 0.01882 0.03730 = 0.01227 0.00502 0.00046 0.00266 AFIX 137 H16A 2 0.520273 0.260113 0.836266 11.00000 -1.50000 H16B 2 0.631734 0.185388 0.862611 11.00000 -1.50000 H16C 2 0.468896 0.131141 0.850580 11.00000 -1.50000 AFIX 0 C17 1 0.618285 0.004774 0.746482 11.00000 0.02050 0.01976 = 0.02140 0.00839 -0.00677 -0.00078 AFIX 137 H17A 2 0.643444 -0.026952 0.695920 11.00000 -1.50000 H17B 2 0.542622 -0.049838 0.760956 11.00000 -1.50000 H17C 2 0.700501 0.014855 0.780924 11.00000 -1.50000 AFIX 0 C18 1 0.762347 0.340263 0.534648 11.00000 0.01140 0.01269 = 0.01697 0.00448 0.00044 0.00068 AFIX 13 H18 2 0.665084 0.313836 0.511483 11.00000 -1.20000 AFIX 0 C19 1 0.867992 0.276415 0.483429 11.00000 0.01513 0.01787 = 0.01697 0.00300 0.00329 0.00040 AFIX 137 H19A 2 0.853263 0.287460 0.432521 11.00000 -1.50000 H19B 2 0.852222 0.192231 0.483906 11.00000 -1.50000 H19C 2 0.964459 0.309687 0.501877 11.00000 -1.50000 AFIX 0 C20 1 0.801006 0.476087 0.539146 11.00000 0.01981 0.01509 = 0.02827 0.00934 0.00439 0.00273 AFIX 137 H20A 2 0.897813 0.502180 0.559557 11.00000 -1.50000 H20B 2 0.737025 0.517992 0.571426 11.00000 -1.50000 H20C 2 0.792310 0.492864 0.489261 11.00000 -1.50000 AFIX 0 C21 1 1.107362 0.138584 0.066500 11.00000 0.01213 0.01192 = 0.01066 0.00573 0.00026 0.00418 C22 1 1.208399 0.294286 0.172741 11.00000 0.01108 0.01414 = 0.01333 -0.00019 -0.00237 -0.00145 C23 1 1.331010 0.246361 0.127810 11.00000 0.01081 0.01784 = 0.01651 0.00373 -0.00052 0.00108 AFIX 23 H23A 2 1.376052 0.194061 0.154100 11.00000 -1.20000 H23B 2 1.402940 0.312162 0.121473 11.00000 -1.20000 AFIX 0 C24 1 1.264199 0.176508 0.050495 11.00000 0.01263 0.01533 = 0.01324 0.00232 0.00178 0.00189 C25 1 1.198454 0.425752 0.172969 11.00000 0.01852 0.01352 = 0.02095 0.00085 -0.00223 -0.00025 AFIX 137 H25A 2 1.190512 0.436743 0.121670 11.00000 -1.50000 H25B 2 1.283020 0.475277 0.198466 11.00000 -1.50000 H25C 2 1.115572 0.447939 0.198916 11.00000 -1.50000 AFIX 0 C26 1 1.220309 0.279407 0.254813 11.00000 0.01746 0.02044 = 0.01416 -0.00006 -0.00316 -0.00108 AFIX 137 H26A 2 1.221868 0.196384 0.255787 11.00000 -1.50000 H26B 2 1.139472 0.305942 0.280913 11.00000 -1.50000 H26C 2 1.307084 0.326532 0.279397 11.00000 -1.50000 AFIX 0 C27 1 1.264795 0.259629 -0.007215 11.00000 0.01646 0.01991 = 0.01528 0.00509 0.00218 -0.00068 AFIX 137 H27A 2 1.361838 0.285558 -0.018064 11.00000 -1.50000 H27B 2 1.220496 0.328325 0.013761 11.00000 -1.50000 H27C 2 1.212420 0.216624 -0.053181 11.00000 -1.50000 AFIX 0 C28 1 1.344205 0.072186 0.018254 11.00000 0.01353 0.01987 = 0.02249 0.00235 0.00588 0.00423 AFIX 137 H28A 2 1.297063 0.028266 -0.028924 11.00000 -1.50000 H28B 2 1.344693 0.019825 0.053601 11.00000 -1.50000 H28C 2 1.441057 0.103012 0.009853 11.00000 -1.50000 AFIX 0 C29 1 0.938045 0.221584 0.160908 11.00000 0.00966 0.01319 = 0.00990 -0.00204 -0.00048 0.00080 C30 1 0.892379 0.158110 0.217533 11.00000 0.01249 0.01570 = 0.00999 -0.00035 -0.00092 0.00003 C31 1 0.771288 0.186876 0.256000 11.00000 0.01744 0.02112 = 0.01528 0.00342 0.00416 0.00146 AFIX 43 H31 2 0.740656 0.146416 0.293874 11.00000 -1.20000 AFIX 0 C32 1 0.696044 0.273716 0.239245 11.00000 0.01465 0.02447 = 0.01993 -0.00039 0.00617 0.00575 AFIX 43 H32 2 0.618015 0.293873 0.266953 11.00000 -1.20000 AFIX 0 C33 1 0.737410 0.330475 0.181053 11.00000 0.01637 0.01681 = 0.02008 0.00033 0.00004 0.00683 AFIX 43 H33 2 0.683735 0.386632 0.168728 11.00000 -1.20000 AFIX 0 C34 1 0.857250 0.306418 0.140011 11.00000 0.01384 0.01331 = 0.01256 -0.00137 -0.00226 0.00121 C35 1 0.958360 0.052933 0.235958 11.00000 0.01440 0.01755 = 0.01115 0.00374 0.00210 0.00195 AFIX 13 H35 2 1.044451 0.044347 0.207250 11.00000 -1.20000 AFIX 0 C36 1 0.849120 -0.061458 0.210600 11.00000 0.01933 0.01816 = 0.01965 0.00509 0.00444 0.00153 AFIX 137 H36A 2 0.816691 -0.067839 0.158804 11.00000 -1.50000 H36B 2 0.768884 -0.057784 0.242261 11.00000 -1.50000 H36C 2 0.893484 -0.130274 0.214879 11.00000 -1.50000 AFIX 0 C37 1 0.998988 0.066317 0.320540 11.00000 0.02172 0.02727 = 0.01270 0.00699 0.00095 0.00368 AFIX 137 H37A 2 1.045879 0.000129 0.327752 11.00000 -1.50000 H37B 2 0.913935 0.067033 0.348659 11.00000 -1.50000 H37C 2 1.062578 0.140167 0.338145 11.00000 -1.50000 AFIX 0 C38 1 0.882640 0.367163 0.072646 11.00000 0.01769 0.01761 = 0.01349 0.00270 0.00004 0.00728 AFIX 13 H38 2 0.968090 0.341962 0.048174 11.00000 -1.20000 AFIX 0 C39 1 0.753592 0.326655 0.015109 11.00000 0.02226 0.02790 = 0.01607 0.00140 -0.00373 0.01049 AFIX 137 H39A 2 0.775775 0.353998 -0.030814 11.00000 -1.50000 H39B 2 0.671899 0.360028 0.035937 11.00000 -1.50000 H39C 2 0.732425 0.240616 0.004230 11.00000 -1.50000 AFIX 0 C40 1 0.904582 0.505198 0.094728 11.00000 0.02718 0.01827 = 0.02214 0.00694 0.00122 0.00793 AFIX 137 H40A 2 0.920036 0.537976 0.050096 11.00000 -1.50000 H40B 2 0.986447 0.532498 0.129761 11.00000 -1.50000 H40C 2 0.820945 0.531199 0.118097 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad in P-1 REM R1 = 0.0277 for 7082 Fo > 4sig(Fo) and 0.0333 for all 8018 data REM 425 parameters refined using 0 restraints END WGHT 0.0330 1.0510 REM Highest difference peak 0.439, deepest hole -0.281, 1-sigma level 0.050 Q1 1 0.7633 0.3237 0.5756 11.00000 0.05 0.44 Q2 1 0.2985 0.2313 0.5619 11.00000 0.05 0.39 Q3 1 0.6202 0.1633 0.7285 11.00000 0.05 0.39 Q4 1 0.3691 0.1612 0.5411 11.00000 0.05 0.37 Q5 1 1.2682 0.2174 0.0254 11.00000 0.05 0.37 Q6 1 0.6638 0.2248 0.6804 11.00000 0.05 0.36 Q7 1 1.1883 0.1618 0.0563 11.00000 0.05 0.36 Q8 1 0.5521 0.1558 0.7883 11.00000 0.05 0.36 Q9 1 1.2048 0.3578 0.1689 11.00000 0.05 0.36 Q10 1 0.3433 0.3010 0.6200 11.00000 0.05 0.35 Q11 1 0.8709 0.3391 0.1091 11.00000 0.05 0.35 Q12 1 0.2571 0.1259 0.5134 11.00000 0.05 0.35 Q13 1 0.3162 0.2151 0.4975 11.00000 0.05 0.35 Q14 1 1.2756 0.2822 0.1529 11.00000 0.05 0.34 Q15 1 0.9819 0.0647 0.2762 11.00000 0.05 0.34 Q16 1 0.4932 0.0839 0.5359 11.00000 0.05 0.34 Q17 1 0.8204 0.3147 0.5107 11.00000 0.05 0.34 Q18 1 0.7839 0.4021 0.5379 11.00000 0.05 0.34 Q19 1 1.0514 0.0827 0.0338 11.00000 0.05 0.33 Q20 1 0.4038 0.3322 0.6806 11.00000 0.05 0.33 ; _shelx_res_checksum 42913 _shelx_hkl_file ; -1 0 0 146.89 5.40 -1 0 0 153.08 5.60 -1 0 0 144.69 5.40 -1 0 0 146.09 5.90 -1 0 0 148.09 5.90 -1 0 0 147.39 5.80 -1 0 0 165.98 5.40 -1 0 0 159.28 5.60 -1 0 0 146.09 5.60 1 0 0 151.98 5.40 1 0 0 144.09 5.80 1 0 0 150.98 5.90 1 0 0 153.08 5.40 1 0 0 146.89 5.60 1 0 0 144.09 5.90 1 0 0 151.48 5.60 1 0 0 151.38 5.50 1 0 0 155.28 5.90 1 0 0 151.88 5.60 -2 0 0 6.30 2.20 -2 0 0 7.10 2.20 -2 0 0 6.50 1.60 -2 0 0 6.40 2.10 -2 0 0 8.10 2.10 -2 0 0 6.60 1.80 -2 0 0 9.60 2.20 -2 0 0 6.30 1.60 -2 0 0 8.70 1.90 -2 0 0 5.60 1.80 2 0 0 6.40 1.50 2 0 0 5.40 1.90 2 0 0 5.90 1.80 2 0 0 4.00 1.80 2 0 0 9.50 2.30 2 0 0 5.70 1.90 2 0 0 10.40 2.30 2 0 0 8.50 1.60 2 0 0 5.40 2.20 2 0 0 6.30 2.10 -3 0 0 47.00 4.00 -3 0 0 55.79 4.90 -3 0 0 55.29 4.10 -3 0 0 66.79 5.10 -3 0 0 57.49 4.30 -3 0 0 44.10 4.40 3 0 0 50.49 3.80 3 0 0 58.69 4.70 3 0 0 55.79 4.20 3 0 0 51.99 4.50 3 0 0 54.09 3.80 3 0 0 58.39 4.90 3 0 0 53.19 4.90 -4 0 0 239.48 11.20 -4 0 0 227.88 9.60 -4 0 0 222.48 11.10 -4 0 0 212.78 9.90 -4 0 0 224.38 9.50 -4 0 0 210.38 10.90 4 0 0 250.37 9.60 4 0 0 229.18 9.40 4 0 0 226.78 11.30 4 0 0 238.18 10.60 4 0 0 204.78 10.30 4 0 0 234.98 10.00 4 0 0 204.08 10.70 -5 0 0 80.79 7.30 -5 0 0 73.39 5.30 -5 0 0 73.29 6.00 -5 0 0 55.09 6.20 -5 0 0 84.79 7.50 5 0 0 71.09 6.00 5 0 0 72.89 6.50 5 0 0 81.09 6.80 5 0 0 77.19 5.10 5 0 0 83.89 6.70 -6 0 0 33.30 5.40 -6 0 0 47.70 6.20 -6 0 0 44.40 5.40 -6 0 0 41.60 6.10 -6 0 0 47.70 4.80 6 0 0 46.30 6.10 6 0 0 46.50 5.30 6 0 0 46.90 5.70 6 0 0 40.90 5.50 6 0 0 50.29 4.60 -7 0 0 195.18 10.70 -7 0 0 190.18 12.00 -7 0 0 176.58 11.80 -7 0 0 188.98 9.60 -7 0 0 189.18 12.00 7 0 0 148.29 10.80 7 0 0 192.08 10.60 7 0 0 162.98 11.50 7 0 0 187.58 11.20 7 0 0 190.98 9.40 -8 0 0 74.99 7.80 -8 0 0 87.19 9.70 -8 0 0 84.99 9.50 8 0 0 73.39 8.40 8 0 0 73.89 8.80 8 0 0 81.19 7.90 8 0 0 86.79 8.90 8 0 0 81.99 6.60 -9 0 0 19.00 5.20 -9 0 0 15.30 5.80 -9 0 0 27.70 6.60 9 0 0 11.80 5.20 9 0 0 14.10 4.70 9 0 0 16.50 5.90 9 0 0 20.50 5.70 -10 0 0 362.06 18.60 -10 0 0 350.96 20.10 -10 0 0 346.27 20.40 10 0 0 340.47 18.90 10 0 0 335.87 19.00 -11 0 0 14.20 7.00 -11 0 0 14.70 6.60 11 0 0 4.90 5.90 11 0 0 6.00 5.50 11 -1 0 24.40 7.20 11 -1 0 29.40 7.00 -11 1 0 24.30 7.20 -11 1 0 13.40 7.00 10 -1 0 112.89 11.10 10 -1 0 110.89 10.80 10 -1 0 121.09 12.10 -10 1 0 109.19 12.20 -10 1 0 124.29 11.20 -10 1 0 138.59 13.40 9 -1 0 43.40 7.60 9 -1 0 48.90 7.50 9 -1 0 42.80 6.90 9 -1 0 56.29 7.50 -9 1 0 39.40 7.50 -9 1 0 58.79 8.50 -9 1 0 49.80 7.00 8 -1 0 120.39 9.90 8 -1 0 128.59 10.40 8 -1 0 121.59 9.50 8 -1 0 122.19 9.40 -8 1 0 124.79 11.40 -8 1 0 116.79 9.10 -8 1 0 131.59 10.60 -8 1 0 127.09 8.20 7 -1 0 66.69 7.60 7 -1 0 59.69 5.00 7 -1 0 47.00 6.00 7 -1 0 61.69 6.70 7 -1 0 57.69 6.90 -7 1 0 53.39 7.00 -7 1 0 68.09 6.00 -7 1 0 64.89 7.60 -7 1 0 73.19 7.10 -7 1 0 61.39 7.60 6 -1 0 213.78 10.90 6 -1 0 215.28 9.20 6 -1 0 194.68 11.20 6 -1 0 192.38 11.50 6 -1 0 199.68 10.80 -6 1 0 218.28 11.90 -6 1 0 215.58 12.00 -6 1 0 221.78 11.00 -6 1 0 201.68 10.00 -6 1 0 195.38 11.70 5 -1 0 4.50 2.90 5 -1 0 -0.40 2.40 5 -1 0 4.40 2.80 5 -1 0 3.00 2.70 5 -1 0 1.50 1.70 -5 1 0 3.20 3.00 -5 1 0 7.70 2.00 -5 1 0 -0.70 2.70 -5 1 0 5.80 2.50 -5 1 0 2.60 2.90 -5 1 0 1.60 2.60 4 -1 0 7.70 2.70 4 -1 0 8.90 2.70 4 -1 0 4.90 2.50 4 -1 0 7.70 1.80 4 -1 0 9.80 3.10 4 -1 0 5.60 2.80 -4 1 0 5.90 3.00 -4 1 0 8.00 2.50 -4 1 0 5.90 2.40 -4 1 0 2.30 2.70 -4 1 0 8.30 1.80 -4 1 0 4.30 2.70 3 -1 0 6.40 2.40 3 -1 0 6.30 2.10 3 -1 0 7.90 1.60 3 -1 0 6.70 2.70 3 -1 0 8.00 2.50 3 -1 0 4.40 1.90 3 -1 0 5.10 2.20 -3 1 0 7.40 2.80 -3 1 0 1.10 2.30 -3 1 0 6.60 1.50 -3 1 0 10.90 2.30 -3 1 0 3.90 2.40 -3 1 0 3.30 2.20 2 -1 0 566.94 20.50 2 -1 0 608.04 20.70 2 -1 0 568.44 20.20 2 -1 0 619.24 21.40 2 -1 0 613.74 21.30 2 -1 0 633.54 21.20 2 -1 0 638.94 20.00 2 -1 0 628.24 20.80 2 -1 0 628.94 21.50 -2 1 0 606.84 19.90 -2 1 0 592.44 20.60 -2 1 0 596.14 20.40 -2 1 0 623.04 21.40 -2 1 0 620.74 20.70 -2 1 0 591.64 21.10 -2 1 0 596.24 21.30 -2 1 0 641.24 20.00 -2 1 0 595.74 21.40 -2 1 0 588.04 20.70 1 -1 0 263.47 9.40 1 -1 0 260.17 9.20 1 -1 0 250.17 9.10 1 -1 0 270.47 9.30 1 -1 0 260.07 8.90 1 -1 0 242.18 9.30 1 -1 0 252.17 8.40 1 -1 0 248.98 9.40 1 -1 0 262.27 8.70 1 -1 0 247.28 9.30 -1 1 0 269.67 8.40 -1 1 0 257.97 8.70 -1 1 0 261.17 9.30 -1 1 0 256.37 9.20 -1 1 0 253.77 9.20 -1 1 0 262.67 8.90 0 -1 0 4303.37 140.49 0 -1 0 4582.34 142.49 0 -1 0 4388.66 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25.20 7 -5 3 597.64 21.70 -8 5 -3 67.79 9.00 -8 5 -3 63.19 7.00 -8 5 -3 73.09 9.10 8 -5 3 76.39 6.80 8 -5 3 74.79 9.00 8 -5 3 71.79 8.60 8 -5 3 69.99 8.40 8 -5 3 79.59 9.10 -9 5 -3 144.49 12.70 -9 5 -3 190.78 13.90 9 -5 3 171.08 12.60 9 -5 3 178.48 13.00 9 -5 3 185.48 13.40 9 -5 3 168.68 12.70 -10 5 -3 54.49 9.10 -10 5 -3 44.10 8.60 10 -5 3 63.09 9.30 10 -5 3 55.19 8.90 10 -5 3 55.89 8.80 10 -5 3 53.69 8.90 -11 5 -3 64.59 10.10 -11 5 -3 52.79 10.10 11 -5 3 49.99 9.00 11 -5 3 61.89 9.90 11 -5 3 65.89 10.30 11 -5 3 54.79 9.10 10 4 -3 41.20 7.60 10 4 -3 31.90 8.20 -10 -4 3 26.50 8.10 -10 -4 3 27.40 8.10 9 4 -3 60.59 8.30 9 4 -3 53.59 8.80 9 4 -3 59.29 8.10 -9 -4 3 55.29 9.40 -9 -4 3 51.49 9.40 8 4 -3 67.89 9.20 8 4 -3 95.69 9.40 8 4 -3 90.19 9.70 -8 -4 3 101.79 9.20 -8 -4 3 101.99 9.20 -8 -4 3 94.19 10.80 -8 -4 3 94.99 10.80 7 4 -3 733.13 30.70 7 4 -3 756.12 29.50 7 4 -3 735.03 31.10 -7 -4 3 784.72 32.20 -7 -4 3 799.22 29.60 -7 -4 3 767.62 32.70 -7 -4 3 778.52 30.20 -7 -4 3 771.12 32.40 6 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15.60 3 10 -9 310.37 16.30 3 10 -9 304.77 18.50 3 10 -9 319.57 18.70 -3 -10 9 296.87 18.10 -3 -10 9 286.97 16.80 -3 -10 9 323.87 18.80 -3 -10 9 300.27 16.30 2 10 -9 9.70 5.20 2 10 -9 15.20 4.70 2 10 -9 14.50 5.90 -2 -10 9 19.00 5.90 -2 -10 9 20.10 5.40 -2 -10 9 8.10 4.40 -2 -10 9 18.90 6.40 1 10 -9 -0.50 3.80 1 10 -9 7.10 4.60 -1 -10 9 -1.40 3.90 -1 -10 9 -2.30 3.20 -1 -10 9 3.90 4.00 -1 -10 9 0.10 4.10 0 10 -9 109.59 10.80 0 10 -9 106.59 11.00 0 -10 9 105.59 8.50 0 -10 9 98.29 10.50 0 -10 9 104.19 10.20 -1 10 -9 351.56 19.60 -1 10 -9 386.06 20.30 -1 10 -9 379.06 18.80 1 -10 9 369.06 19.50 1 -10 9 403.66 20.20 1 -10 9 370.16 16.70 1 -10 9 360.36 17.20 -2 10 -9 260.77 14.60 -2 10 -9 234.58 15.40 -2 10 -9 268.67 16.00 2 -10 9 253.57 15.20 2 -10 9 272.27 13.70 2 -10 9 251.77 15.70 2 -10 9 239.18 13.10 -3 10 -9 66.59 9.20 -3 10 -9 62.29 7.30 -3 10 -9 49.70 7.80 3 -10 9 27.20 6.50 3 -10 9 50.89 6.30 3 -10 9 54.89 8.30 3 -10 9 50.09 6.90 -4 10 -9 25.20 6.90 -4 10 -9 29.40 6.50 4 -10 9 16.00 6.00 4 -10 9 31.70 6.90 4 -10 9 22.20 4.90 4 -10 9 13.60 5.00 -5 10 -9 201.88 14.30 -5 10 -9 210.88 15.10 -5 10 -9 210.08 13.90 5 -10 9 175.38 11.70 5 -10 9 210.98 13.80 5 -10 9 191.38 14.30 -6 10 -9 0.40 4.90 -6 10 -9 -3.00 4.50 -6 10 -9 2.30 4.80 6 -10 9 1.30 4.80 6 -10 9 3.10 3.90 6 -10 9 -5.20 4.20 -7 10 -9 374.16 22.30 -7 10 -9 385.16 22.10 7 -10 9 369.26 19.40 7 -10 9 367.36 21.60 7 -10 9 379.96 21.20 -8 10 -9 14.40 7.20 -8 10 -9 8.80 5.90 8 -10 9 7.10 6.50 8 -10 9 7.70 5.20 8 -10 9 10.80 6.80 7 9 -9 223.18 16.90 7 9 -9 199.98 15.50 -7 -9 9 197.18 16.30 -7 -9 9 245.68 17.20 -7 -9 9 178.88 15.50 -7 -9 9 232.08 16.50 6 9 -9 15.80 6.20 6 9 -9 11.70 6.30 -6 -9 9 0.40 5.20 -6 -9 9 11.20 6.70 -6 -9 9 7.20 5.70 5 9 -9 317.77 19.60 5 9 -9 305.47 17.50 5 9 -9 334.47 19.20 -5 -9 9 285.57 18.10 -5 -9 9 321.37 19.30 -5 -9 9 329.37 18.60 4 9 -9 10.00 5.20 4 9 -9 6.80 5.20 4 9 -9 -5.10 3.70 -4 -9 9 -5.80 4.20 -4 -9 9 3.80 4.90 -4 -9 9 1.60 4.10 -4 -9 9 -0.70 3.90 3 9 -9 333.07 18.90 3 9 -9 320.07 18.60 3 9 -9 351.26 17.20 -3 -9 9 322.47 18.70 -3 -9 9 342.17 18.70 -3 -9 9 342.17 17.40 -3 -9 9 359.26 17.10 2 9 -9 106.29 8.70 2 9 -9 107.89 10.80 2 9 -9 109.49 11.10 -2 -9 9 113.29 9.20 -2 -9 9 104.79 10.70 -2 -9 9 100.49 8.50 -2 -9 9 122.79 11.90 1 9 -9 30.20 6.00 1 9 -9 28.10 5.00 1 9 -9 31.00 6.40 -1 -9 9 23.00 5.80 -1 -9 9 33.60 5.60 -1 -9 9 32.90 6.30 -1 -9 9 32.30 5.20 0 9 -9 176.68 9.80 0 9 -9 181.78 11.80 0 9 -9 149.49 11.80 0 9 -9 180.68 12.40 0 -9 9 177.58 10.20 0 -9 9 162.48 11.50 0 -9 9 153.18 12.60 0 -9 9 163.58 9.20 -1 9 -9 12.20 4.80 -1 9 -9 13.40 4.50 -1 9 -9 -0.20 3.90 1 -9 9 5.50 3.90 1 -9 9 5.00 3.40 1 -9 9 5.20 4.30 1 -9 9 2.80 3.00 -2 9 -9 6.10 4.30 -2 9 -9 4.40 4.20 -2 9 -9 -1.20 3.10 2 -9 9 7.60 3.30 2 -9 9 3.80 3.80 2 -9 9 4.30 3.40 2 -9 9 4.10 4.10 -3 9 -9 459.55 21.60 -3 9 -9 475.15 19.80 -3 9 -9 441.86 22.00 3 -9 9 464.25 20.20 3 -9 9 436.06 18.80 3 -9 9 387.56 21.00 3 -9 9 420.86 21.00 -4 9 -9 3.50 4.10 -4 9 -9 -1.30 3.90 -4 9 -9 1.70 4.20 4 -9 9 6.00 4.40 4 -9 9 5.20 2.90 4 -9 9 10.90 3.80 4 -9 9 7.00 4.30 -5 9 -9 670.43 30.30 -5 9 -9 683.23 29.00 -5 9 -9 625.34 29.90 5 -9 9 656.13 28.60 5 -9 9 701.93 30.10 5 -9 9 654.43 27.00 5 -9 9 696.33 26.00 -6 9 -9 11.50 5.70 -6 9 -9 16.00 5.40 -6 9 -9 15.00 5.80 6 -9 9 20.60 6.50 6 -9 9 19.00 5.00 6 -9 9 14.00 4.60 6 -9 9 18.80 6.30 -7 9 -9 344.37 20.60 -7 9 -9 364.46 21.20 7 -9 9 368.76 18.10 7 -9 9 380.96 18.80 7 -9 9 322.37 19.70 7 -9 9 377.76 21.10 -8 9 -9 -4.70 4.90 -8 9 -9 4.70 5.30 8 -9 9 8.50 6.10 8 -9 9 0.70 4.60 8 -9 9 5.60 4.90 8 -9 9 0.20 5.40 -9 9 -9 56.29 10.30 -9 9 -9 31.80 8.40 9 -9 9 35.30 8.80 9 -9 9 43.40 8.00 9 -9 9 37.00 8.00 9 -9 9 30.00 8.30 8 8 -9 9.20 6.50 8 8 -9 4.30 5.70 -8 -8 9 2.40 6.20 -8 -8 9 6.10 7.00 -8 -8 9 8.80 6.60 -8 -8 9 0.10 6.60 7